SWIM decided to write up a theoretical report on how to extract alkaloids from p harmala and decided to include some theoretical GC-MS data. Remember this is theoretical and was not and should not be performed where these alkaloids are controlled substances.
Objective: To extract Harmine and Harmaline from Peganum harmala.
Methods:
1- 100 gram seeds powdered in blender.
2- Immersed in 400 mL distilled water made acidic with 5 drops glacial acetic acid.
Let stand overnight. Stirred occasionally.
3- Heated extract for about 1 hour and then filtered through cotton wool and a buchner funnel with vacuum.
4- Added 300 mL hot acidic dH2O (10 drops acetic acid).
Let stand overnight with occasional stirring.
5- Filtered same way as above. Pooled filtrates.
6- Added another 300 mL hot acidified dH2O. Let stand for about 1 hour with occasional stirring. Filtered same way as above.
7- The pooled filtrates were then filtered through glass fiber filter with sea sand (previously cleaned with HCl) through a buchner funnel under vacuum. There by 600 mL of filtrate was obtained. Note this is less water then started with so some residual water was left in the seed mush.
8- To this was added 60 grams NaCl to make 10% salt solution. The solution was then boiled down to 300 mL to make a 20% salt solution and stored in 4 degrees C over a weekend. In retrospect the solution should have been boiled down then salt added. Note the solution turned dark brown after concentrating.
9- The precipitant observed was filtered through filter paper in a buchner funnel under vacuum and allowed to dry over night.
10- 1.5 grams of crude alkaloids was thus obtained. It was a brown residue clearly impure with brown solid particles mixed with crystalline alkaloids.
11- The crude alkaloid extract was then dissolved in 60 mL hot water and immediately filtered to remove the solid impurities.
12- To this solution 6 grams NaCl was added to make a 10% salt solution. This solution was stored at 4 degrees C for a few hours.
13- Alkaloid precipitation was observed. Alkaloids were filtered again with filter paper and buchner funnel under vacuum. The alkaloids were dried over night.
14- Thus a yield of 1 gram alkaloids was obtained as a light brown crystalline powder. Edit: The 60 mL of filtrate was chilled a second time and more alkaloids precipitates so yield more like 1.2g.
15- Purity was analyzed by GC-MS. Only 2 peaks were observed in a concentrated analytical sample. Harmine was the major component along with harmaline as a minor component.
Overall this represents a 1% total yield. In the literature p harmala is said to have 2-7% alkaloids. However some of these alkaloids are not harmine or harmaline. SWIM would like to discuss a literature report that concerns the alkaloids in p harmala in another thread.
Objective: To extract Harmine and Harmaline from Peganum harmala.
Methods:
1- 100 gram seeds powdered in blender.
2- Immersed in 400 mL distilled water made acidic with 5 drops glacial acetic acid.
Let stand overnight. Stirred occasionally.
3- Heated extract for about 1 hour and then filtered through cotton wool and a buchner funnel with vacuum.
4- Added 300 mL hot acidic dH2O (10 drops acetic acid).
Let stand overnight with occasional stirring.
5- Filtered same way as above. Pooled filtrates.
6- Added another 300 mL hot acidified dH2O. Let stand for about 1 hour with occasional stirring. Filtered same way as above.
7- The pooled filtrates were then filtered through glass fiber filter with sea sand (previously cleaned with HCl) through a buchner funnel under vacuum. There by 600 mL of filtrate was obtained. Note this is less water then started with so some residual water was left in the seed mush.
8- To this was added 60 grams NaCl to make 10% salt solution. The solution was then boiled down to 300 mL to make a 20% salt solution and stored in 4 degrees C over a weekend. In retrospect the solution should have been boiled down then salt added. Note the solution turned dark brown after concentrating.
9- The precipitant observed was filtered through filter paper in a buchner funnel under vacuum and allowed to dry over night.
10- 1.5 grams of crude alkaloids was thus obtained. It was a brown residue clearly impure with brown solid particles mixed with crystalline alkaloids.
11- The crude alkaloid extract was then dissolved in 60 mL hot water and immediately filtered to remove the solid impurities.
12- To this solution 6 grams NaCl was added to make a 10% salt solution. This solution was stored at 4 degrees C for a few hours.
13- Alkaloid precipitation was observed. Alkaloids were filtered again with filter paper and buchner funnel under vacuum. The alkaloids were dried over night.
14- Thus a yield of 1 gram alkaloids was obtained as a light brown crystalline powder. Edit: The 60 mL of filtrate was chilled a second time and more alkaloids precipitates so yield more like 1.2g.
15- Purity was analyzed by GC-MS. Only 2 peaks were observed in a concentrated analytical sample. Harmine was the major component along with harmaline as a minor component.
Overall this represents a 1% total yield. In the literature p harmala is said to have 2-7% alkaloids. However some of these alkaloids are not harmine or harmaline. SWIM would like to discuss a literature report that concerns the alkaloids in p harmala in another thread.
